Solid-phase microextraction coupled to liquid chromatography for the analysis of phenolic compounds in water

Solid-phase microextraction (SPME) coupled to high-performance liquid chromatography (HPLC) has been applied to the analysis of priority pollutant phenolic compounds in water samples. Two types of polar fibers [50 microm Carbowax-templated resin (CW-TPR) and 60 microm polydimethylsiloxane-divinylbenzene (PDMS-DVB)] were evaluated. The effects of equilibration time and ionic strength of samples on the adsorption step were studied. The parameters affecting the desorption process, such as desorption mode, solvent composition and desorption time, were optimized. The developed method was used to determine the phenols in spiked river water samples collected in the Douro River, Portugal. Detection limits of 1-10 microg l(-1) were achieved under the optimized conditions.     

Determination of hydroxyaromatic compounds in water by solid-phase microextraction coupled to high-performance liquid chromatography

Solid-phase microextraction (SPME) coupled with high-performance liquid chromatography (HPLC) for the analysis of hydroxyaromatic compounds is described. Three kinds of fibers [50 microns carbowax-templated resin (CW-TPR), 60 microns polydimethylsiloxane-divinylbenzene (PDMS-DVB) and 85 microns polyacrylate (PA) fibers] were evaluated. CW-TPR and PDMS-DVB were selected for further study. The parameters of the desorption procedure (such as desorption mode, the composition of the solvent for desorption and the duration of fiber soaking) were studied and optimized. The effect of the structure and physical properties of analytes, carryover, duration of absorption, temperature of absorption, pH and ionic strength of samples were also investigated. The method was applied to environmental samples (lake water) using a simple calibration curve.     

Determination of chlorophenols by solid-phase microextraction and liquid chromatography with electrochemical detection

A solid-phase microextraction method has been developed for the determination of 19 chlorophenols (CPs) in environmental samples. The analytical procedure involves direct sampling of CPs from water using solid-phase microextraction (SPME) and determination by liquid chromatography with electrochemical detection (LC-ED). Three kinds of fibre [50 microm carbowax-templated resin (CW-TPR), 60 microm polydimethylsiloxane-divinylbenzene (PDMS-DVB) and 85 microm polyacrylate (PA)] were evaluated for the analysis of CPs. Of these fibres, CW-TPR is the most suitable for the determination of CPs in water. Optimal conditions for both desorption and absorption SPME processes, such as composition of the desorption solvent (water-acetonitrile-methanol, 20:30:50) and desorption time (5 min), extraction time (50 min) and temperature (40 degrees C) as well as pH (3.5) and ionic strength (6 g NaCl) were established. The precision of the SPME-LC-ED method gave relative standard deviations (RSDs) of between 4 and 11%. The method was linear over three to four orders of magnitude and the detection limits, from 3 to 8 ng l(-1), were lower than the European Community legislation limits for drinking water. The method was applied to the analysis of CPs in drinking water and wood samples.     

Solid-phase microextraction coupled with high-performance liquid chromatography for the analysis of heterocyclic aromatic amines

Solid-phase microextraction (SPME) coupled with high-performance liquid chromatography (HPLC) with UV diode array detection (DAD) for the analysis of heterocyclic aromatic amines (HAs) is described. Four kinds of fiber coatings: Carbowax-templated resin (CW-TPR), Carbowax-divinylbenzene (CW-DVB), poly(dimethylsiloxane)-divinylbenzene (PDMS-DVB) and polyacrylate (PA) were evaluated for extraction of nine most biologically active heterocyclic aromatic amines. Different parameters affecting to the microextraction and determination of HAs were studied, such as absorption and desorption time, desorption mode, composition of the solvent for desorption, pH, ionic strength, and percentage of methanol in the sample. To determine these amines in food samples a new simplified procedure is proposed, consisting of treatment of the sample with methanolic NaOH prior microextraction by CW-TPR fiber coating and HPLC-DAD determination. The advantages of this new method are the reduced amounts of time and organic solvents required.     

Surface energy characteristics of toner particles by automated inverse gas chromatography

This study develops a method for the analysis of biocides Irgarol 1051 and Sea Nine 211 in environmental water samples, using solid-phase microextraction (SPME). Their determination was carried out using gas chromatography with flame thermionic (FTD), electron-capture (ECD) and mass spectrometric detection. The main parameters affecting the SPME process such as adsorption-time profile, salt additives and memory effect were studied for five polymeric coatings commercially available for solid-phase microextraction: poly(dimethylsiloxane) (100 and 30 microm), polyacrylate, poly(dimethylsiloxane)-divinylbenzene (PDMS-DVB 65 microm) and Carbowax-divinylbenzene (65 microm). The method was developed using spiked natural waters such as tap, river, sea and lake water in a concentration range of 0.5-50 microg/l. All the tested fiber coatings have been evaluated with regard to sensitivity, linear range, precision and limits of detection. Typical RSD values (triplicate analysis) in the range of 3-10% were obtained depending on the fiber coating and the compound investigated. The recoveries of biocides were in relatively high levels 60-118% and the calibration curves were reproducible and linear (R2>0.990) for both analytes. The SPME partition coefficients (Kf) of both compounds were also calculated experimentally in the proposed conditions for all fibers using direct sampling. Finally the influence of organic matter such as humic acids on extraction efficiency was studied, affecting mostly Sea Nine 211 uptake by the fiber. Optimum analytical SPME performance was achieved using the PDMS-DVB 65 microm fiber coating in ECD and FTD systems for Sea Nine 211 and Irgarol 1051, respectively.     

Multiresidue method for the simultaneous determination of four groups of pesticides in ground and drinking waters,using solid-phase microextraction-gas chromatography with electron-capture and thermionic specific detection

A common sample preparation procedure capable of efficiently concentrating various groups of pesticides, taking advantage of universal detectors like the mass spectrometer or combined techniques of group selective detectors like gas chromatography-electron capture detection (ECD)/thermionic specific detection (TSD), is desirable in environmental analysis. Six solid-phase microextraction fibres available for analysis of semi-volatiles (7, 30 and 100 microm poly(dimethylsiloxane) (PDMS), 85 microm polyacrylate, 60 microm PDMS-divinylbenzene (PDMS-DVB) and 65 microm Carbowax-DVB) were evaluated and the 60 microm PDMS-DVB was selected for the simultaneous extraction of 34 compounds, included in the organochlorine (OCPs), organophosphorous (OPPs), pyrethroid and triazine pesticide groups. All parameters affecting the extraction efficiency from water samples, namely fibre coating, sample agitation, pH and ionic strength, extraction temperature and time, were optimised. The analytical procedure involves solid-phase microextraction extraction, gas chromatographic separation and subsequent ECD and TSD via a post-column splitter adjusted to a split ratio of 1:10, respectively. Detection limits in the range of 1-10 ng l(-1) for OCPs, 1-30 ng l(-1) for OPPs, 20-30 ng l(-1) for pyrethroids and 8-50 ng l(-1) for triazines are easily attainable with the optimised procedure. The method validated for ground and drinking waters has low cost of implementation and operation although it requires careful maintenance.     

Development of a sensitive methodology for the analysis of chlorobenzenes in air by combination of solid-phase extraction and headspace solid-phase microextraction

In this study, a combination of solid-phase extraction (SPE) and solid-phase microextraction (SPME) has been used to determine chlorobenzenes in air. Analytes were sampled by pumping a known volume of air through a porous polymer (Tenax TA). Then, the adsorbent was transferred into a glass vial and SPME was performed. The quantification was carried out using gas chromatography (GC)-electron-capture detection or GC-MS. Several SPME coatings (100 microm poly(dimethylsiloxane) (PDMS), 75 microm Carboxen (CAR)-PDMS, 65 microm PDMS-divinylbenzene (DVB), 65 microm PDMS-DVB and 85 microm polyacrylate (PA) were evaluated, obtaining the highest responses with Carbowax (CW)- PDMS for the most volatile chlorobenzenes, and with PDMS-DVB or CW-DVB fibers for the semivolatile compounds. To optimize some other factors that could affect the SPME step, a factorial design was used. Kinetic studies of the SPME process were also performed. Concerning the SPE step, breakthrough was studied, showing that 2.5 m3 of air could be processed without losses of the most volatile compounds. The performance of the method was evaluated. External calibration, which does not require the complete sampling process, demonstrated to be suitable, obtaining good linearity (R2 > 0.99) for all chlorobenzenes. Recovery studies were performed at two concentration levels (4 and 40 ng/m3), obtaining quantitative recoveries (>80%). Limits of detection at the sub ng/m3 were achieved for all the target compounds.     

Glass nebulizer interface for capillary electrophoresis-Fourier transform infrared spectrometry

Despite the continuing development of SPME (solid-phase microextraction) fibre coatings, their selection presents some difficulties for analysts in choosing the appropriate fibre for a certain application. There are two distinct types of SPME coatings available commercially. The most widely used are poly(dimethylsiloxane) (PDMS) and poly(acrylate) (PA). Supelco has developed new mixed phases consisting of porous polymer particles, either poly(divinylbenzene) (DVB) or Carboxen suspended in a matrix of PDMS or Carbowax for extracting analytes via adsorption. In addition to the nature of the extracting phase, the thickness of the polymeric film must be taken into account and, surprisingly, the construction of the fibres when apparently they bear the same coating, as it is the case of the three PDMS-DVB fibres available. Other fibre structure properties not well explored were identified and must be taken into consideration. To elucidate their extraction efficiency, three PDMS-DVB fibres, namely 60 microm for HPLC use, 65 microm for GC use and 65 microm StableFlex for GC use, were compared with regard to the extraction of 36 compounds included in four pesticide groups. The first was particularly suited for the extraction of organophosphorus pesticides and triazines whereas the StableFlex exhibited advantages in the analysis of organochlorine pesticides and pyrethroids. An explanation for the extraction differences is suggested based on the different structure of the fibres. Detection limits in the range of 1-10 ng/l for organochlorine pesticides, 1-30 ng/l for organophosphorus pesticides, 8-50 ng/l for triazines and 10-20 ng/l for pyrethroids were attained in a method using the 60 microm PDMS-DVB fibre. The fibre maintains its performance at well above 100 extractions with between-day precision below 10%.     

Simultaneous analysis of polychlorinated biphenyls and organochlorine pesticides in water by headspace solid-phase microextraction with gas chromatography-tandem mass spectrometry

Headspace solid-phase microextraction combined with gas chromatography-ion trap tandem mass spectrometry (HS-SPME-GC-ITMS-MS) method has been developed and studied for the simultaneous determination of 15 organochlorine pesticides (OCPs) and 20 polychlorinated biphenyls (PCBs) in aqueous samples. To perform the HS-SPME polydimethylsiloxane (PDMS) (7, 30 and 100 microm film thickness) and polydimethylsiloxane-divinylbenzene (PDMS-DVB) fibers were initially compared on the basis of their absorption capacities for the selected compounds, and PDMS 100 microm film thickness was selected to accomplish the rests of essays. The influence of various parameters on OCPs and PCBs extraction efficiency by HS-SPME was thoroughly studied using GC-electron capture detector (ECD). Parameters such as collision induced dissociation (CID) resonant excitation amplitude and RF storage level were optimized to increase specificity and sensibility for ITMS-MS analysis. The performance of proposed HS-SPME-GC-ITMS-MS methodology with respect to linearity, reproducibility and limit of detection (LOD) was evaluated by water spiked with target compounds. The linear range of most compounds was found to be between 0.01 and 1 ng mL(-1) and the limits of detection were between 0.4 and 26 pg mL(-1). The reproducibility of the method (n = 6), expressed as relative standard deviation (RSD), was between 5 and 21%. Finally, developed procedure was applied to determine selected OCPs and PCBs in river water samples in concentration below 0.1 ng mL(-1) can be easily carried out with ultra-selectivity and precision.     

Optimisation of solid-phase microextraction coupled to HPLC-UV for the determination of organochlorine pesticides and their metabolites in environmental liquid samples

A solid-phase microextraction (SPME) procedure using two commercial fibers coupled with high-performance liquid chromatography (HPLC) is presented for the extraction and determination of organochlorine pesticides in water samples. We have evaluated the extraction efficiency of this kind of compound using two different fibers: 60-μm polydimethylsiloxane–divinylbenzene (PDMS-DVB) and Carbowax/TPR-100 (CW/TPR). Parameters involved in the extraction and desorption procedures (e.g. extraction time, ionic strength, extraction temperature, desorption and soaking time) were studied and optimized to achieve the maximum efficiency. Results indicate that both PDMS-DVB and CW/TPR fibers are suitable for the extraction of this type of compound, and a simple calibration curve method based on simple aqueous standards can be used. All the correlation coefficients were better than 0.9950, and the RSDs ranged from 7% to 13% for 60-μm PDMS-DVB fiber and from 3% to 10% for CW/TPR fiber. Optimized procedures were applied to the determination of a mixture of six organochlorine pesticides in environmental liquid samples (sea, sewage and ground waters), employing HPLC with UV-diode array detector.     

Optimization of headspace solid-phase microextraction gas chromatography-atomic emission detection analysis of monomethylmercury

Optimum conditions for headspace solid-phase microextraction (HS-SPME) in the analysis of monomethylmercury (MeHg) have been determined. Sodium tetra(n-)propylborate (NaBPr(4)) is used as derivatization reagent to promote volatility. A simple aluminium bar was used to cool the SPME fiber to about 2 degrees C during the equilibration phase just before extraction. HS-SPME was performed using different fibers. The 100 microm polydimethylsiloxane (PDMS) and 65 microm polydimethylsiloxane-divinylbenzene (PDMS-DVB) fibers showed the best results. Although the extraction efficiency for MeHg derivative of the polydimethylsiloxane-Carboxen (PDMS-CAR) fiber is similar to the other fibers, desorption of MeHg derivative from a PDMS-CAR fiber is poor. Factors affecting the HS-SPME process such as adsorption and desorption times, ionic strength (salting-out) and extraction temperature have been evaluated and optimized thoroughly. The highest extraction efficiency for the PDMS fiber was obtained by extraction at a low temperature (2 degrees C) immediately after equilibration at 30 degrees C. With the PDMS-DVB and PDMS-CAR fiber improvement of extraction efficiency at lower temperatures is negligible. Repeated extraction out of the same vial revealed that about 30% of MeHg derivative is extracted from the headspace with a PDMS fiber at 2 degrees C and about 70% with a PDMS-DVB fiber. Repeated extraction with two different fiber coatings showed that the PDMS-CAR fiber also extracts about 70% but that the desorption is incomplete. Attempts to improve the desorption failed due to degradation of the MeHg derivate at high injection temperatures. The limit of detection (3sigma) was 16 pg/L MeHg. The relative standard deviation (n = 8) for 100 pg/L of MeHg was found to be 5%. Linearity of the HS-SPME-GC-atomic emission detection method was established over at least two orders of magnitude in the range 0-2000 pg/L. Recovery of a surface water sample spiked at 2 ng/L was 85%. The suitability of the procedure was demonstrated by analysis of a surface water sample that showed a concentration of 100 pg/L MeHg. The optimized method can be used with standard commercial equipment without further adaptations.     

Comparison of different fibers for the solid-phase microextraction of phthalate esters from water

Solid-phase microextraction (SPME) coupled to gas chromatography-mass spectrometry (GC-MS) has been applied to determine six phthalate esters and one adipate ester in water. The SPME parameters were optimized for several commercially available fibers. A 65-microm polydimethylsiloxane-divinylbenzene (PDMS-DVB) was the fiber selected and was applied to analysis of water from the Ebro river and the industrial port of Tarragona. The studied compounds were found at concentrations ranging from 0.4 microg l(-1) for di-n-butyl phthalate ester (DnBP) to 3.2 microg l(-1) for bis(2-ethylhexyl) phthalate ester (DEHP). The linear range for real samples was from 0.1 to 10 microg l(-1) for most phthalates, and the limits of detection of the method were between 3 and 30 ng l(-1). Repeatability and reproducibility between days (n = 5) for 1 microg l(-1) samples were below 13 and 18%, respectively.     

Multivariate optimization of a solid-phase microextraction method for the analysis of phthalate esters in environmental waters

A solid-phase microextraction method (SPME) coupled to gas chromatography-mass spectrometry (GC-MS) has been developed for the determination of the six phthalate esters included in the US Environmental Protection Agency (EPA) Priority Pollutants list in water samples. These compounds are dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), butylbenzyl phthalate (BBP), di-2-ethylhexyl phthalate (DEHP) and di-n-octyl phthalate (DOP). Detailed discussion of the different parameters, which could affect the extraction process, is presented. Main factors have been studied and optimized by means of a multifactor categorical design. Different commercial fibers, polydimethylsiloxane (PDMS), polydimethylsiloxane-divinylbenzene (PDMS-DVB), polyacrylate (PA), Carboxen-polydimethylsiloxane (CAR-PDMS) and Carbowax-divinylbenzene (CW-DVB), have been investigated, as well as the extraction mode, exposing the fiber directly into the sample (DSPME) or into the headspace over the sample (HS-SPME), and different extraction temperatures. The use of this experimental design allowed for the evaluation of interactions between factors. Extraction kinetics has also been studied. The optimized microextraction method showed linear response and good precision for all target analytes. Detection limits were estimated considering the contamination problems associated to phthalate analysis. They were in the low pg mL(-1), excluding DEHP (100 pg mL(-1)). The applicability of the developed SPME method was demonstrated for several real water samples including mineral, river, industrial port and sewage water samples. All the target analytes were found in real samples. Levels of DEP and DEHP were over 1 ng mL(-1) in some of the samples.     

Simultaneous determination of phenyl- and sulfonyl-urea herbicides in river water at sub-parts-per-billion level by on-line preconcentration and liquid chromatography-tandem mass spectrometry

A method based on solid-phase microextraction and gas chromatography flame photometric detector for the determination of organophosphorus pesticides (OPPs) in food samples was described. Three kinds of vinyl crown ether polar fibers were prepared with sol-gel process and used for the analytes. The new coatings showed higher extraction efficiency and sensitivity for organophosphorus pesticides compared with commercial fibers—85 μm PA and 65 μm PDMS-DVB. Specifically, the benzo-15-crown-5 coating was the most effective for the target analytes. Several factors affecting the performance of SPME such as extraction temperature and time, salt addition, and dilution ratios of samples were optimized. The apparent recoveries of spiked food samples (apple juice, apple and tomato) were determined to be over 55.3% and the limits of detection (LODs) were in the range of 0.003-0.09 ng/g for the OPP studied. The method was applied to determine the concentrations of OPP in real food samples.     

Highly porous solid-phase microextraction fiber coating based on poly(ethylene glycol)-modified ormosils synthesized by sol-gel technology

The preparation and characteristics of solid-phase microextraction (SPME) fibers coated with Carbowax 20M ormosil (organically modified silica) are described here. Raw fused silica fibers were coated with Carbowax 20M-modified silica using sol-gel process. Scanning electron micrographs of fibers revealed a highly porous, sponge-like coating with an average thickness of (8 +/- 1) microm. The sol-gel Carbowax fibers were compared to commercial fibers coated with 100 microm polydimethylsiloxane (PDMS) and 65 microm Carbowax-divinylbenzene (DVB). Shorter equilibrium times were possible with the sol-gel Carbowax fiber: for headspace extraction of the test analytes, they ranged from less than 3 min for benzene to 15 min for o-xylene. Extraction efficiencies of the sol-gel Carbowax fiber were superior to those of conventional fibers: for o-xylene, the extracted masses were 230 and 540% of that obtained with 100 microm PDMS and 65 microm Carbowax-DVB fibers, respectively.     

Fibre selection based on an overall analytical feature comparison for the solid-phase microextraction of trihalomethanes from drinking water

This paper describes the optimization of solid-phase microextraction (SPME) conditions for three different fibres (Carboxen-polydimethylsiloxane (CAR-PDMS), divinylbenzene-Carboxen-polydimethylsiloxane (DVB-CAR-PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB)) used to determine trihalomethanes (THMs) in water by headspace solid-phase microextraction and gas chromatography (HS-SPME-GC). The influence of temperature and salting-out effect was examined using a central composite design for each fibre. Extraction time was studied separately at the optimum values found for temperature and sodium chloride concentration (40 degrees C and 0.36g mL-1). The HS-SPME-GC-MS method for each fibre was characterised in terms of linearity, detection (LOD) and quantification (LOQ) limits and repeatability. The fibre PDMS-DVB was selected as it provided a broader linear range, better repeatability and lower detection and quantification limits than the others, particularly CAR-PDMS fibre. The accuracy of the proposed method using the PDMS-DVB fibre was checked by a recovery study in both ultrapure and tap water. A blank analysis study showed the absence of memory effects for this fibre. The reproducibility (expressed as a percentage of relative standard deviation) was 6-11% and the detection limits were between 0.078 and 0.52microgL-1 for bromoform and chloroform, respectively. Finally, the method was applied to determine THM concentration in two drinking water samples.     

Preparation and application of NiTi alloy coated with ZrO(2) as a new fiber for solid-phase microextraction

In this study a NiTi alloy was applied as an SPME support due to its superelasticity and shape memory properties. This new metallic support was coated with ZrO(2) by electrodeposition using chronoamperometry. It was then evaluated for extraction of three classes of compounds from gaseous samples: alcohols, BTEX and trihalomethanes (THM). For the optimization of the parameters affecting the extraction efficiency of the target compounds, the univariate approach was used. Five fibers were electrodeposited to evaluate the reproducibility of the coating procedure, resulting in a relative standard deviation lower than 11.9%. The repeatability for one fiber (n=6) was lower than 8.5%. The detection limits were lower than 28.1, 20.8 and 0.18 microgL(-1) for alcohols, BTEX and THM, respectively, and the correlation coefficients were higher than 0.996. Taking into account the amount extracted per unit volume, the NiTi-ZrO(2) fiber showed a better extraction profile in comparison with the commercial fibers 7 microm PDMS, 85 microm PA and 30-50 microm DVB/CAR/PDMS. The new SPME fiber has a lifetime of over 300 extractions. Thus, it is a promising alternative for low-cost analysis, as it is robust, and easily and inexpensively prepared.     

Studies on the aroma of cupuassu liquor by headspace solid-phase microextraction and gas chromatography

Headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography with ion trap mass spectrometric detection and with atomic emission detection (GC-AED) was employed to identify possible odor-impact volatile organic compounds in cupuassu (Theobroma grandiflorum Spreng) liquor, as well as to quantify alkylpyrazines present in these samples. SPME fibers coated with 100 microm polydimethylsiloxane (PDMS), 65 microm PDMS-divinylbenzene (DVB) and 75 microm Carboxen (CAR)-PDMS were tested, the later being chosen for the optimized extraction procedure. The principal compounds found in the sample headspace were 3-methylbutanal, dimethylsulfide, dimethyldisulfide, beta-linalool and several alkylpyrazines (notably tetramethylpyrazine). The procedure for quantitation of the alkylpyrazines, using GC-AED for their separation and detection, allowed the detection of microg g(-1) levels of the analytes in the samples, with acceptable precision (R.S.D. less than 10%).     

Hollow fiber membrane-protected solid-phase microextraction of triazine herbicides in bovine milk and sewage sludge samples

A porous polypropylene hollow fiber membrane (HFM)-protected solid-phase microextraction (HFM-SPME) procedure in conjunction with gas chromatography/mass spectrometric analysis for use in the determination of triazine herbicides in bovine milk samples is described. A 65-microm polydimethylsiloxane-divinylbenzne (PDMS-DVB) SPME fiber was protected by an HFM. HFM-SPME experimental parameters such as fiber type, extraction time, extraction temperature and salt concentration were investigated and optimized. The relative standard deviations for the reproducibility of the optimized HFM-SPME method varied from 4.30 to 12.37%. The correlation coefficients of the calibration curves were between 0.9799 and 0.9965 across a concentration range of 0-200 microg l(-1). The method detection limits for triazines in bovine milk were in the range of 0.003-0.013 microg l(-1) and limits of quantification were in the range of 0.006-0.021 microg l(-1). The suitability of HFM-SPME was extended to the analysis of the herbicides in sewage sludge samples. The results demonstrate that HFM-SPME was an efficient pretreatment and enrichment procedure for complex matrices.     

Solid Phase Microextraction Fibers Coated with Sol-gel Aminopropylsilica/polydimethylsiloxane: Development and Its Application to Screening of Beer Headspace

The preparation and applicability of solid phase microextraction (SPME) fibers coated with a sol-gel organically modified silica based on 3-aminopropyltrimethoxysilane and polydimethylsiloxane (APTMS/PDMS) are described here. Micrographs of the coated fibers revealed a rugous surface; the thickness of the coating was estimated to be less than 30 microm. The APTMS/PDMS fibers were tested with synthetic samples and compared to commercial fibers for headspace SPME analysis of beer. Extraction and desorption using the APTMS/PDMS fibers were faster, which is typical for sol-gel SPME fibers. For polar and semi-polar compounds on beer headspace, the extraction efficiencies of the APTMS/PDMS fiber were superior to those of conventional fibers. The APTMS/PDMS fiber was found to be capable of extracting a broad range of analytes, including highly polar acidic species such as organic acids.